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Hydrochloric Acid → HCID 67005686、化合物

HRID 564289
ノート
印刷プレビュー

反応式

HRID 564289 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]2[N:6]=[CH:7][S:8][C:4]=2[CH:3]=1.N1C=CC=CC=1.[C:17]([NH:25][C:26]1[CH:27]=[C:28]([CH:32]=[CH:33][CH:34]=1)[C:29](Cl)=[O:30])(=[O:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl>O1CCCC1.C(OCC)(=O)C>[S:8]1[C:4]2[CH:3]=[C:2]([NH:1][C:29](=[O:30])[C:28]3[CH:32]=[CH:33][CH:34]=[C:26]([NH:25][C:17](=[O:24])[C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=4)[CH:27]=3)[CH:10]=[CH:9][C:5]=2[N:6]=[CH:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 682886-AminobenzothiazoleHCID 184700593-Benzamidobenzoyl chloride

生成物 1

HCID 67005686HCID 67005686、化合物収率 60.3%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution of 0.1 g of 6-aminobenzothiazole and 0.1 g of pyridine added to 5 ml of tetrahydrofuran and stirred at room temperature was introduced dropwise 0.2 g of 3-(benzoylamino)benzoyl chloride dissolved in 1 ml of tetrahydrofuran. The resulting solution was stirred at room temperature for 1 hour, and then ethyl acetate and 1N hydrochloric acid were added thereto for separating the organic phase. The organic phase was washed with saturated sodium hydrogen carbonate solution one time, and then dried over anhydrous magnesium sulfate. The solution was filtered off, the filtrate was collected, and the solvent was removed under a reduced pressure to obtain a residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1) to obtain 0.15 g of the desired product (Yield: 52%) as a white solid.

後処理

  1. stirringThe resulting solution was stirred at room temperature for 1 hour
  2. customfor separating the organic phase
  3. washThe organic phase was washed with saturated sodium hydrogen carbonate solution one time
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe solution was filtered off
  6. customthe filtrate was collected
  7. customthe solvent was removed under a reduced pressure
  8. customto obtain a residue
  9. customThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-7d742ced661e432cbf55e82b4c071c9f
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08067638B2

反応ノート

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